CN115611307A - Preparation method of anatase titanium dioxide special for chemical fibers - Google Patents

Preparation method of anatase titanium dioxide special for chemical fibers Download PDF

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CN115611307A
CN115611307A CN202211345401.1A CN202211345401A CN115611307A CN 115611307 A CN115611307 A CN 115611307A CN 202211345401 A CN202211345401 A CN 202211345401A CN 115611307 A CN115611307 A CN 115611307A
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titanium
discharging
tank
titanium dioxide
washing
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刘震
李勇
陈海梅
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Xuzhou Titanium Dioxide Chemical Co ltd
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Xuzhou Titanium Dioxide Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/65Chroma (C*)

Abstract

The invention relates to a preparation method of anatase chemical fiber special titanium dioxide, belonging to the technical field of titanium dioxide production, and controlling the F value of titanium liquid to be 1.9 +/-5 in the acidolysis process. The temperature of first boiling and second boiling in the hydrolysis process is controlled, so that the uniform particle size distribution of the metatitanic acid hydrolysis aggregate is ensured. Controlling Fe during water washing 2 O 3 The content (ppm) is less than or equal to 50, the calcining temperature and time are controlled in the calcining process, the moderate hardness is ensured, the particles are crisp and easy to crush, and the content of the discharging kiln is less than or equal to 100ppm; the calcium oxide of the product is less than or equal to 80ppm.

Description

Preparation method of anatase titanium dioxide special for chemical fibers
Technical Field
The invention belongs to the technical field of titanium dioxide production, and particularly relates to a preparation method of anatase type special titanium dioxide for chemical fibers.
Background
Titanium dioxide, generally referred to as titanium dioxide, is a white inorganic pigment having no toxicity, optimal opacity, optimal whiteness and brightness, and is considered to be the best performing white pigment in the world today. The titanium white has strong adhesive force, is not easy to cause chemical change and is always snow white. It can be widely used in the industries of paint, plastics, paper making, printing ink, chemical fiber, rubber, cosmetics, etc. It has high melting point, and can be used for making refractory glass, glaze, enamel, pottery clay, high-temperature-resistant experimental ware, etc. Titanium dioxide is stable in nature, is used in large quantities as a white pigment in paints, has good hiding power, is similar to white lead, but does not turn black like white lead; it has the same durability as zinc white. Titanium dioxide is also used as a matting agent for enamels and can produce a very bright, hard and acid-resistant enamel cover coat.
However, in the existing titanium dioxide preparation process, the prepared titanium dioxide has low whiteness, low decolorization and higher oil absorption.
Chinese patent CN202110307144.1 discloses a production process for increasing whiteness of titanium dioxide, comprising the following steps: s1, raw material treatment: adding ilmenite into a grinder for grinding, performing coarse-fine separation on the ilmenite through a winnowing machine after grinding, returning unqualified ilmenite to the grinder for reprocessing, and conveying qualified ilmenite powder into a storage bin for storage; s2, acidolysis treatment: adding the powder prepared in the step S1 into an acidolysis tank, adding sulfuric acid with the concentration of 91-95% into the acidolysis tank, uniformly stirring, introducing steam into the acidolysis tank, carrying out acidolysis reaction on the material under the action of the steam, standing for a period of time after the acidolysis reaction, adding water into the acidolysis tank, leaching and extracting the material by water, and obtaining a titanium solution after the extraction is finished; s3, settling treatment: conveying the titanium liquid into a sedimentation tank, adding a flocculating agent into the tank, and precipitating insoluble impurities and colloidal particles in the titanium liquid through the flocculating agent; s4, cooling and crystallizing, namely adding the titanium liquid into cooling and impurity removing equipment to remove iron in the titanium liquid, performing sedimentation treatment to obtain a large amount of soluble impurities which mainly exist in a ferrous sulfate form, cooling the titanium liquid by using a cooling medium to ensure that the ferrous sulfate in the solution is in a saturated state, and then separating out the ferrous sulfate along with the reduction of the temperature; s5, subsequent processing: after the treatment of soluble impurities and insoluble impurities in the titanium liquid is finished, adding the titanium liquid into a hydrolysis tank for hydrolysis treatment, obtaining hydrated titanium dioxide after the hydrolysis treatment is finished, then washing and bleaching the hydrated titanium dioxide, finally calcining the hydrated titanium dioxide, and crushing the calcined material after the treatment is finished, thus obtaining the titanium dioxide.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of special anatase titanium dioxide for chemical fibers.
The purpose of the invention can be realized by the following technical scheme:
the preparation method of the anatase titanium dioxide special for chemical fibers comprises the following steps:
s1, placing raw ores into an air swept mill for crushing, then sending the crushed raw ores into a classifier for sorting, sending qualified mineral powder into a mineral powder bin after sorting, removing dust by using a bag-type dust remover in the process, then sending the qualified mineral powder into a premixing tank through a mineral powder weighing hopper, stirring and adding concentrated sulfuric acid, discharging the mixture into an acid hydrolysis tank after uniformly stirring, adding a starting acid to initiate a main reaction, adding process water for leaching after the reaction is finished for curing time, then adding iron powder for reduction, and discharging the prepared precipitated titanium liquid into a settling pond after trivalent titanium appears;
s2, adding a flocculating agent into a sedimentation tank for sedimentation, discharging upper-layer titanium clear liquid after sedimentation, discharging lower-layer substrate into a hot-pressing filter, adding process water for filter pressing, discharging the upper-layer titanium clear liquid after standing, collecting the twice-discharged titanium clear liquid, discharging the twice-discharged titanium clear liquid into a crystallizer, discharging the twice-discharged titanium clear liquid into a crystalline titanium liquid tank after vacuum crystallization, filtering ferrous sulfate by a disc to obtain crude titanium liquid, discharging the fine-filtered titanium clear liquid into a titanium clear liquid tank, and discharging concentrated liquid into a concentrated storage tank after concentration;
s3, discharging the concentrated solution in the concentrated storage tank into a hydrolysis tank for hydrolysis, adding cellulose serving as authigenic seed crystal, and preparing metatitanic acid after hydrolysis;
s4, washing the prepared metatitanic acid, performing salt treatment, discharging into a salt treatment storage tank, performing filter pressing through a filter press to obtain treated metatitanic acid, and feeding into a rotary kiln for calcination;
and S5, cooling after calcining, crushing and grinding by a Raymond mill, and packaging by an anatase bag filter to obtain the anatase type titanium dioxide special for chemical fibers.
Further: in the step S1, the fineness of the qualified mineral powder is less than or equal to 45 mu m, and the screen residue is 5-12%.
Further: the stirring mode of the premixing tank in the step S1 is compressed air stirring, and the flow rate of the compressed air is adjusted to>800m 3 /h
Further, the method comprises the following steps: the starting acid in the step S1 is sulfuric acid with the mass fraction of 92.5 percent, and when a solid phase substance is matureThe time is 60min, the leaching reduction time is 6h, and the process water flow is 1560-1585kg/m 3
Further, the method comprises the following steps: in the step S2, the flocculating agent is 7504 flocculating agent, and the using amount is 0.5 per mill.
Further: the washing in step S4 includes primary washing, bleaching and secondary washing.
Further: the washing method comprises the following specific steps: washing metatitanic acid with deionized water for the first time (to remove soluble impurities), pulping, adding sulfuric acid, stirring at a constant speed, adding a reducing agent, reducing, washing with deionized water for the second time, and pulping to obtain a slurry.
Further, the method comprises the following steps: s4, the salt treatment process comprises the steps of conveying the metatitanic acid after water washing into a salt treatment tank, adding a salt treatment agent through a salt solution head tank, wherein the salt treatment agent is a composite salt, and the composite salt accounts for 0.5% (by K) 2 O/TiO 2 Calculated as P) potassium carbonate and 0.3% (calculated as P) 2 O 5 /TiO 2 Meter) phosphoric acid.
The invention has the beneficial effects that:
the method controls the F value of the titanium liquid to be 1.9 +/-5 in the acidolysis process. The primary boiling (106.5 ℃) and the secondary boiling (108.5 ℃) are controlled in the hydrolysis process, and the uniform particle size distribution of the hydrolyzed metatitanic acid aggregate is ensured. The Fe2O3 content (ppm) is controlled to be less than or equal to 50 in the water washing process, the calcining temperature (950-1050 ℃) and the calcining time (8-10 hours) are controlled in the calcining process, the moderate hardness is ensured, the particles are crisp and easy to crush, and the discharging kiln content is less than or equal to 100ppm. The calcium oxide of the product is less than or equal to 80ppm, and the titanium dioxide with good whiteness, high decolorization and low oil absorption is finally prepared.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a preparation method of anatase type titanium dioxide special for chemical fibers.
FIG. 2 is an electron microscope image of titanium white of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1-2, the invention relates to a method for preparing anatase titanium dioxide special for chemical fiber, comprising the following steps:
s1, placing raw ore in a pneumatic sweeping mill for crushing, then feeding the crushed raw ore into a classifier for sorting, feeding qualified mineral powder into a mineral powder bin after sorting, removing dust by using a bag-type dust remover in the process, then feeding the qualified mineral powder into a premixing tank through a mineral powder weighing hopper, stirring and adding concentrated sulfuric acid, discharging the mixture into an acidolysis tank after uniformly stirring, adding a starting acid to initiate a main reaction, adding process water for leaching after the reaction is finished, then adding iron powder for reduction, and discharging the prepared precipitated titanium liquid into a settling tank after trivalent titanium appears; the quality indexes of the precipitated titanium liquid are shown in the following table 1:
TABLE 1
Figure BDA0003917018140000051
S2, adding a flocculating agent into a sedimentation tank for sedimentation, discharging upper-layer titanium clear liquid after sedimentation, discharging lower-layer substrate into a hot-pressing filter, adding process water for filter pressing, discharging the upper-layer titanium clear liquid after standing, collecting the twice-discharged titanium clear liquid, discharging the twice-discharged titanium clear liquid into a crystallizer, discharging the twice-discharged titanium clear liquid into a crystalline titanium liquid tank after vacuum crystallization, filtering ferrous sulfate by a disc to obtain crude titanium liquid, discharging the fine-filtered titanium clear liquid into a titanium clear liquid tank, and discharging concentrated liquid into a concentrated storage tank after concentration;
s3, discharging the concentrated solution in the concentrated storage tank into a hydrolysis tank for hydrolysis, adding cellulose serving as authigenic seed crystal, and preparing metatitanic acid after hydrolysis;
the indexes of the ferrous sulfate, the crude titanium liquid and the titanium liquid after fine filtration are shown in the following table 2:
TABLE 2
Figure BDA0003917018140000052
Figure BDA0003917018140000061
S4, washing the prepared metatitanic acid, performing salt treatment, discharging into a salt treatment storage tank, performing filter pressing through a filter press to obtain treated metatitanic acid, and feeding into a rotary kiln for calcination;
and S5, cooling after calcining, crushing and grinding by a Raymond mill, and packaging by an anatase bag filter to obtain the anatase type titanium dioxide special for chemical fibers.
The indexes of the anatase titanium dioxide special for chemical fibers prepared in the embodiment 1 are shown in the following table 3:
TABLE 3
Figure BDA0003917018140000062
Figure BDA0003917018140000071
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.

Claims (8)

1. The preparation method of the special anatase titanium dioxide for chemical fiber is characterized by comprising the following steps: the method comprises the following steps:
s1, placing raw ore in a pneumatic sweeping mill for crushing, then feeding the crushed raw ore into a classifier for sorting, feeding qualified mineral powder into a mineral powder bin after sorting, then feeding the qualified mineral powder into a premixing tank through a mineral powder metering hopper, stirring and adding concentrated sulfuric acid, discharging the mixture into an acidolysis tank after uniformly stirring, adding starting acid, curing after the reaction is finished, adding process water for leaching, then adding iron powder, and discharging the prepared precipitated titanium solution into a settling tank after trivalent titanium appears;
s2, adding a flocculating agent into a sedimentation tank for sedimentation, discharging upper-layer titanium clear liquid after sedimentation, discharging lower-layer substrate into a hot-pressing filter, adding process water for filter pressing, discharging the upper-layer titanium clear liquid after standing, collecting the twice-discharged titanium clear liquid, discharging the twice-discharged titanium clear liquid into a crystallizer, discharging the twice-discharged titanium clear liquid into a crystalline titanium liquid tank after vacuum crystallization, filtering ferrous sulfate by a disc to obtain crude titanium liquid, discharging the fine-filtered titanium clear liquid into a titanium clear liquid tank, and discharging concentrated liquid into a concentrated storage tank after concentration;
s3, discharging the concentrated solution in the concentration storage tank into a hydrolysis tank for hydrolysis, adding cellulose, and hydrolyzing to obtain metatitanic acid;
s4, washing the prepared metatitanic acid, performing salt treatment, discharging into a salt treatment storage tank, performing filter pressing through a filter press to obtain treated metatitanic acid, and feeding into a rotary kiln for calcination;
and S5, cooling after calcining, crushing and grinding through a Raymond mill, and packaging to obtain the anatase chemical fiber special titanium dioxide.
2. The preparation method of the anatase type chemical fiber special titanium dioxide according to claim 1, characterized in that: the method is characterized in that: in the step S1, the fineness of the qualified mineral powder is less than or equal to 45 mu m, and the residue on sieve is 5-12%.
3. The preparation method of the anatase type chemical fiber special titanium dioxide according to claim 1, characterized in that: the method is characterized in that: the stirring mode of the premixing tank in the step S1 is compressed air stirring, and the flow rate of the compressed air is adjusted to>800m 3 /h。
4. The preparation method of the anatase type chemical fiber special titanium dioxide according to claim 1, characterized in that: the method is characterized in that: in the step S1, the starting acid is sulfuric acid with the mass fraction of 92.5%, the maturation time of a solid phase substance is 60min, the leaching reduction time is 6h, and the process water flow is 1560-1585kg/m 3
5. The preparation method of the anatase type chemical fiber special titanium dioxide according to claim 1, characterized in that: the method is characterized in that: in the step S2, the flocculating agent is 7504 flocculating agent, and the using amount is 0.5 per mill.
6. The method for preparing the anatase titanium dioxide special for chemical fibers according to claim 1, wherein the method comprises the following steps: the method is characterized in that: the washing in step S4 includes primary washing, bleaching and secondary washing.
7. The method for preparing the anatase type chemical fiber special titanium dioxide according to claim 6, characterized in that: the method is characterized in that: the washing method comprises the following specific steps: washing metatitanic acid with deionized water for the first time (to remove soluble impurities), pulping, adding sulfuric acid, stirring at a constant speed, adding a reducing agent, reducing, washing with deionized water for the second time, and pulping to obtain a slurry.
8. The method for preparing the anatase type chemical fiber special titanium dioxide according to claim 7, characterized in that: the method is characterized in that: and S4, the salt treatment process is to send the washed metatitanic acid into a salt treatment tank, and add a salt treatment agent through a salt solution head tank, wherein the salt treatment agent is a composite salt, and the composite salt is 0.5% of potassium carbonate and 0.3% of phosphoric acid.
CN202211345401.1A 2022-10-31 2022-10-31 Preparation method of anatase titanium dioxide special for chemical fibers Pending CN115611307A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1850619A (en) * 2006-05-12 2006-10-25 南京钛白化工有限责任公司 Method for preparing anatase chemical fiber special titanium pigment
CN102627321A (en) * 2012-04-01 2012-08-08 沙立林 Method for preparing titanium pigment by using titanium residues obtained by directly reducing titanium-iron oxide
CN113044880A (en) * 2021-03-23 2021-06-29 江苏勃仑化学有限公司 Production process for increasing whiteness of titanium dioxide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1850619A (en) * 2006-05-12 2006-10-25 南京钛白化工有限责任公司 Method for preparing anatase chemical fiber special titanium pigment
CN102627321A (en) * 2012-04-01 2012-08-08 沙立林 Method for preparing titanium pigment by using titanium residues obtained by directly reducing titanium-iron oxide
CN113044880A (en) * 2021-03-23 2021-06-29 江苏勃仑化学有限公司 Production process for increasing whiteness of titanium dioxide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王杏: "《纳米二氧化钛的生产与应用》", vol. 2014, 贵州科技出版社, pages: 36 - 39 *

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